During FY16, the Clinical Pharmacology Program (CPP) provided support to over 90 clinical trials. This support ranged from sample pickup and processing, to full analytical method development and validation, pharmacokinetic and pharmacogenetic analysis and assistance with trial design. In FY16, the CPP processed over 30,000 biological samples including blood, urine and ascites. Upon arrival, all samples are processed, barcoded and frozen for future use. The first priority in characterizing the pharmacokinetics of an anticancer agent is to develop a reliable and reproducible analytical method for quantitating agents in biological fluids and tissues. The CPP utilizes high performance liquid chromatography (HPLC) coupled with state-of-the-art detection instruments including mass spectrometers, tandem mass spectrometers (MS/MS), diode array detectors (for UV absorption), and fluorescence detection to measure drug concentrations. Following method development, assays are validated according to the FDA Guidelines for Bioanalytical Method Development. Over the years, the CPP has developed analytical methods for a wide range of therapeutics, numerous which have been published, including depsipeptide, TNP-470, phenylacetate, phenylbutyrate, tamoxifen, UCN-01, CAI, thalidomide, COL-3, suramin, melphalan, erlotinib, perifosine, SU5416, 2ME, MS-275, ketoconazole, lenalidomide, romidepsin, AZD2281 and gemicitabine, sorafenib, finasteride, nelfinavir, 17-DMAG, clopidogrel and and its MPB-derivatized active thiol-metabolite (CAMD), Hsp90 inhibitor PF-04928473, irinotecan (its active metabolite SN38, and glucuronidated SN38), Trk kinase inhibitor AZD7451, pomalidomide, olaparib, sorafenib, belinostat, cediranib, abiraterone, cabozantinib, carfilzomib, midazolam, lapatinib, temozolomide, perifosine, and valproic acid. We have recently developed a sensitive and selective ultra-high performance liquid chromatography-tandem mass spectrometric method for the quantification of temozolomide (TMZ) in nonhuman primate (NHP) plasma, cerebrospinal fluid (CSF), and brain extracellular fluid (ECF) following microdialysis.